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1. 沈阳化工学院 稀土化学及应用辽宁省高校重点实验室,辽宁 沈阳,110142
2. 东北大学 材料冶金学院,辽宁 沈阳,110004
收稿日期:2008-08-25,
修回日期:1900-01-02,
网络出版日期:2009-04-30,
纸质出版日期:2009-04-30
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周 岩, 肖林久, 贺明睿, 等. 溶胶-凝胶法制备BaGd1-xEuxB9O16红色磷光粉的发光[J]. 发光学报, 2009,30(2):189-194.
Structure and Luminescence Properties of BaGdBaGd1-xEuxB9O16 Phosphor Prepared by Sol-gel Method[J]. Chinese journal of luminescence, 2009, 30(2): 189-194.
采用溶胶-凝胶法制备出BaGd
1-x
Eu
x
B
9
O
16
红色磷光粉
对过程的物料配比、前驱体处理和晶化温度等制备条件进行了讨论。结果表明
样品在850 ℃下开始晶化
900 ℃时就能够获得较好的晶化产物
结合不同晶化温度下的发光强度比较确定
晶化温度为950 ℃时
BaGd
1-x
Eu
x
B
9
O
16
磷光粉具有较高的结晶状态和发光强度。当Eu浓度x=0.9时具有最大的发光强度;初始原料配比硼酸须按计量过量15%。所得荧光粉的激发光谱峰值为264
394
465
534 nm等
分别归属于Eu-O电荷迁移带及Eu
3+
的
7
F
0
-
5
L
6
、
7
F
0
-
5
D
2
和
7
F
0
-
5
D
1
跃迁
发射光谱呈Eu
3+
的特征红光
最强的发射峰位于614 nm
归属于
5
D
0
-
7
F
2
跃迁。进一步研究表明该磷光粉中存在着Gd
3+
对Eu
3+
的能量传递。
Rare-earth doped borate phosphor has the advantage of low synthesis temperature
so it is suffered much of recognition in recent decades years. Ba<em>Ln</em>B<sub>9</sub>O<sub>16</sub> (<em>Ln</em>=La-Lu
Y) is a fine borate host
which can gained different phosphors by doping of different ions (Ce
Dy
Eu
Tb
Mn). For the before time investigation of borate phosphor
solid-state method was used for preparing
the fabrication temperature is about 1 000 ℃
and more the phenomenon of agglomeration is very grave. We synthesized a Eu<sup>3+</sup> doped boron-containing phosphor having a formula of BaGd<sub>1-<em>x</em></sub>Eu<sub><</sub>em>x</em>B<sub>9</sub>O<sub>16</sub> by sol-gel method
decreasing the crystallized temperature and avoiding the grave agglomeration.<br>Using Eu<sub>2</sub>O<sub>3</sub>
Gd<sub>2</sub>O<sub>3</sub>
boracic acid
barium carbonate acid as starting materials and citric acid as complexing agent
sol-gel method was used to prepare BaGd<sub>1-<em>x</em></sub>Eu<sub><em>x</em></sub>B<sub>9</sub>O<sub>16</sub> red phosphor. The influence of preparing condition was discussed
and their structure and luminescence property were characterized by X-ray diffraction (XRD) analysis and fluorescence spectrometry. The investigation showed that the sample can be crystallized under 850 ℃
and gained better crystallized production at 900 ℃. Considering to the luminescence intensity for the samples prepared at different crystallization temperature
BaGd<sub>1-<em>x</em></sub>Eu<sub><em>x</em></sub>B<sub>9</sub>O<sub>16</sub> phosphor can get better luminescence intensity and better purity.<p/>The investigation showed that there is huge quenching concentration of Eu<sup>3+</sup> in BaGd<sub>1-<em>x</em></sub>Eu<sub><em>x</em></sub>B<sub>9</sub>O<sub>16</sub>. Its about 90%. For the borate synthesis
boracic acid can be volatilization at high temperature
so 15% excessive boracic was necessary. The investigation found that the phosphor can be excitated by 264
394
465
534 nm; they are assigned to Eu—O energy transfer
<sup>7</sup>F<sub>0</sub>→<sup>5</sup>L<sub>6</sub>
<sup>7</sup>F<sub>0</sub>-<sup>5</sup>D<sub>2</sub>
<sup>7</sup>F<sub>0</sub>-<sup>5</sup>D<sub>1</sub> transitions
respectively. The samples can emit out characteristic red light of Eu<sup>3+</sup> with the main peak of 614 nm
which is assigned to <sup>5</sup>D<sub>0</sub>-<sup>7</sup>F<sub>2</sub> transition. The energy transfer between Gd<sup>3+</sup> and Eu<sup>3+</sup> exist in this phosphor. Different from the phosphors prepared by solid-state method
the highest excitation position is not from energy transfer
it comes from f-f transition which located at 394 nm. Thats suitable to white LED that can give the excitation of purple ray.
. Zhang Guoyou, Zhao Xiaoxia, Meng Qingyu, et al. Preparation and properties of red emitting phosphor Gd2MO3O9 : Eu3+ for white LEDs [J]. Chin. J. Lumin. (发光学报), 2007, 28 (1):57-61 (in Chinese).
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. Pan Jun, Yao Lianzeng, Chen Lingao. Spectrum property of Na5Eu(WO4)4 laser crystal [J]. J. Hebei Hydraulic Engineering College (河北水专学报), 1990, 2 :49-53 (in Chinese).
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. Yang Zhi, Lin Jianhua, Su Mianzeng. Structural and luminescent properties of LnBaB9O16 : Eu3+ (Ln= La,Y) [J]. Chem. J. Chin. Univer. (高等学校化学学报), 1999, 20 (12):1832-1837 (in Chinese).
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